Methanol → 3-[2-Chloro-4-(trifluoromethyl)phenoxy]benzoic acid methyl ester

온도

50 °C

To a 300 ml, 3-necked flask equipped with a stirrer, gas bubbling tube, condenser, thermometer and drying tube is charged anhydrous methanol (100 ml) and 3-(2-chloro-4-trifluoromethylphenoxy)benzoic acid (12 g., 0.038 mole). Anhydrous hydrogen chloride gas is bubbled into the reaction mixture until the reaction temperature (exotherm) rises to 50° C. The reaction mixture is then maintained at 50° C. with external heating for 4 hours, then cooled, the solvent removed in vacuo and the residue dissolved in CCl4 (200 ml) and triturated with water (50 ml). The decanted and dried (anh. MgSO4) CCl4 layer is reduced in vacuo to give 12.2 g. of methyl 3-(2-chloro-4-trifluoromethylphenoxy)benzoate (98% yield).

1. customTo a 300 ml, 3-necked flask equipped with a stirrer
2. customgas bubbling tube, condenser
3. customthermometer and drying tube
4. customAnhydrous hydrogen chloride gas is bubbled into the reaction mixture until the reaction temperature (exotherm)
5. customrises to 50° C
6. temperaturewith external heating for 4 hours
7. temperaturecooled
8. customthe solvent removed in vacuo
9. dissolutionthe residue dissolved in CCl4 (200 ml)
10. customtriturated with water (50 ml)
11. customThe decanted
12. dry with materialdried (anh. MgSO4) CCl4 layer
13. customto give 12.2 g

ORD 기록

ord-934a86f90d964f338bc5f3d4af4a7a79

출처 데이터셋

uspto-grants-1977_06

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US04031131